CN113568234B - Black-high-transmission reversible transition laminated polymer film and preparation method and application thereof - Google Patents
Black-high-transmission reversible transition laminated polymer film and preparation method and application thereof Download PDFInfo
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- CN113568234B CN113568234B CN202110726534.2A CN202110726534A CN113568234B CN 113568234 B CN113568234 B CN 113568234B CN 202110726534 A CN202110726534 A CN 202110726534A CN 113568234 B CN113568234 B CN 113568234B
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- 229920006254 polymer film Polymers 0.000 title claims abstract description 61
- 230000002441 reversible effect Effects 0.000 title claims abstract description 12
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- 230000007704 transition Effects 0.000 title claims description 5
- 239000000178 monomer Substances 0.000 claims abstract description 71
- 229920000642 polymer Polymers 0.000 claims abstract description 34
- 239000002243 precursor Substances 0.000 claims abstract description 27
- 238000006116 polymerization reaction Methods 0.000 claims abstract description 23
- 238000000034 method Methods 0.000 claims abstract description 21
- 238000002484 cyclic voltammetry Methods 0.000 claims abstract description 19
- 239000011521 glass Substances 0.000 claims abstract description 19
- 238000004528 spin coating Methods 0.000 claims abstract description 12
- 230000005540 biological transmission Effects 0.000 claims abstract description 11
- 229920001577 copolymer Polymers 0.000 claims abstract description 10
- 230000003287 optical effect Effects 0.000 claims abstract description 6
- 239000000463 material Substances 0.000 claims description 22
- 238000002834 transmittance Methods 0.000 claims description 15
- 239000002904 solvent Substances 0.000 claims description 9
- 239000003115 supporting electrolyte Substances 0.000 claims description 8
- 229910021607 Silver chloride Inorganic materials 0.000 claims description 2
- 230000001747 exhibiting effect Effects 0.000 claims description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 2
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 3
- 230000007935 neutral effect Effects 0.000 claims 1
- 239000004984 smart glass Substances 0.000 claims 1
- 238000006243 chemical reaction Methods 0.000 abstract description 3
- 230000004044 response Effects 0.000 abstract description 3
- 239000000243 solution Substances 0.000 description 74
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 description 39
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 15
- -1 tetrabutylammonium hexafluorophosphate Chemical compound 0.000 description 12
- 238000010521 absorption reaction Methods 0.000 description 5
- 239000012046 mixed solvent Substances 0.000 description 5
- 239000011149 active material Substances 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 230000001351 cycling effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000006722 reduction reaction Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
Classifications
-
- G—PHYSICS
- G02—OPTICS
- G02F—OPTICAL DEVICES OR ARRANGEMENTS FOR THE CONTROL OF LIGHT BY MODIFICATION OF THE OPTICAL PROPERTIES OF THE MEDIA OF THE ELEMENTS INVOLVED THEREIN; NON-LINEAR OPTICS; FREQUENCY-CHANGING OF LIGHT; OPTICAL LOGIC ELEMENTS; OPTICAL ANALOGUE/DIGITAL CONVERTERS
- G02F1/00—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics
- G02F1/01—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour
- G02F1/15—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour based on an electrochromic effect
- G02F1/1514—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour based on an electrochromic effect characterised by the electrochromic material, e.g. by the electrodeposited material
- G02F1/1516—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour based on an electrochromic effect characterised by the electrochromic material, e.g. by the electrodeposited material comprising organic material
- G02F1/15165—Polymers
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- Physics & Mathematics (AREA)
- Nonlinear Science (AREA)
- General Physics & Mathematics (AREA)
- Optics & Photonics (AREA)
- Electrochromic Elements, Electrophoresis, Or Variable Reflection Or Absorption Elements (AREA)
Abstract
A black-high transmission reversibly switchable laminated polymer film prepared by the method of: firstly, preparing a polymer solution (I) with the concentration of 6mg/mL, uniformly dripping the polymer solution (I) onto FTO conductive glass, and preparing a polymer film by spin coating through a spin coater; secondly, preparing a monomer solution (II) and a monomer solution (III) with the concentration of 1 mg/mL; then, taking a solution with the mass ratio of 2:3-3:2 from the monomer solution (II) and the monomer solution (III) to prepare a precursor solution of a red monomer and a green monomer; finally, a copolymer film is electrodeposited on the FTO conductive glass spin-coated with the polymer film in the precursor solution by using a cyclic voltammetry polymerization method. And a preparation method and application of the laminated polymer film are provided. The invention can realize black-high transmission reversible conversion, and has higher optical contrast and quicker response time.
Description
Technical Field
The invention relates to a black-high-transmission reversible-conversion laminated polymer film, a preparation method and application thereof, and the film can be used as an electrochromic active material and applied to intelligent windows, automobile rearview mirrors, flat panel displays and wearable equipment.
Background
Electrochromic (EC) refers to a phenomenon that a material undergoes oxidation/reduction reaction under an applied voltage, along with charge injection/extraction and ion doping/dedoping, and the color of the material changes reversibly in appearance. When electrochromic materials are fabricated on transparent conductive substrates and a voltage is applied, their color changes can be clearly observed, and the color remains unchanged for a long time after the applied voltage is removed, thus being applicable to the field of energy-saving display. Because electrochromic materials have the advantages of rich colors, low energy consumption and the like, great interest in academia and industry is gradually aroused, and the electrochromic materials show great potential application value in the fields of intelligent windows, automobile rearview mirrors, flat panel displays and flexible wearable.
Among the existing electrochromic materials, black electrochromic materials report relatively few, because black electrochromic materials require that the polymer must achieve full absorption (400 nm-800 nm) of the entire visible region, which has very high requirements for material design and synthesis. In 2008, J.R. Reynolds et al (nature materials,2008,7,795-799) synthesized the first black electrochromic material by adjusting the donor-acceptor structure, however, the disadvantage was that the synthesis process of the material was cumbersome and difficult to control. In 2016, a black-displaying polymer electrochromic material was prepared by a solution blending method as taught by Xu Chunshe in our country (New J.chem,2016,40,5231-5237). The preparation of the material is relatively simple, but the electrochromic performance of the prepared material is poor, and the material is mainly characterized by low optical contrast and low response speed.
Disclosure of Invention
In order to overcome the defects in the prior art, the invention provides a black display polymer film which can realize the reversible conversion of color from black to transparent as an electrochromic material, has high optical contrast, quick response time and good cycling stability; simultaneously, a simple and controllable method for preparing the polymer film is provided; in addition, the prepared polymer film is used as an electrochromic active material to be applied to electrochromic devices such as intelligent windows, automobile rearview mirrors, plane displays and wearable equipment.
The technical scheme adopted for solving the technical problems is as follows:
a black-high transmission reversibly switchable laminated polymer film prepared by the method of: firstly, preparing a polymer solution (I) with the concentration of 1-10 mg/mL, uniformly dripping the polymer solution (I) onto FTO conductive glass, and preparing a polymer film by spin coating through a spin coater; secondly, preparing a monomer solution (II) and a monomer solution (III) with the concentration of 0.5-5 mg/mL; then, taking a solution with the mass ratio of 2:3-3:2 from the monomer solution (II) and the monomer solution (III) to prepare a precursor solution of a red monomer and a green monomer; finally, electrodepositing a layer of copolymer film on the FTO conductive glass spin-coated with the polymer film in the precursor solution by using a cyclic voltammetry polymerization method;
。
further, a polymer solution was prepared using a polymer exhibiting purple color and an electrolytic solvent, and was named as polymer solution (I); uniformly dripping the polymer solution (I) on FTO conductive glass, and preparing a polymer film by spin coating through a spin coater; in a three-electrode system using FTO conductive glass spin-coated with a polymer film as a working electrode, a platinum wire as a counter electrode and an Ag/AgCl electrode as a reference electrode, two polymerization precursors respectively showing red and green, a supporting electrolyte and an electrolytic solvent are used to prepare two monomer solutions, which are respectively named monomer solution (II) and monomer solution (III).
The polymer concentration in the prepared polymer solution is 1-10 mg/mL (preferably 3-8 mg/L); in the prepared monomer solution, the monomer concentration is 0.5-5 mg/mL (preferably 1-3 mg/mL), and the concentration of the supporting electrolyte is 0.05-0.3 mol/L (preferably 0.1-0.2 mol/L).
A method for preparing a black-high transmission reversible transition laminated polymer film, which comprises the following steps: firstly, preparing a polymer solution (I) with the concentration of 1-10 mg/mL, uniformly dripping the polymer solution (I) onto FTO conductive glass, and preparing a polymer film by spin coating through a spin coater; secondly, preparing a monomer solution (II) and a monomer solution (III) with the concentration of 0.5-5 mg/mL; then, taking a solution with the mass ratio of 2:3-3:2 from the monomer solution (II) and the monomer solution (III) to prepare a precursor solution of a red monomer and a green monomer; finally, electrodepositing a layer of copolymer film on the FTO conductive glass spin-coated with the polymer film in the precursor solution by using a cyclic voltammetry polymerization method;
。
the spin speed of the spin coater was 1500rpm and the spin time was 60s.
The electrolytic solvent is a mixed solvent of dichloromethane and acetonitrile according to a volume ratio of 3:2.
The voltage range in the cyclic voltammetry polymerization method is-1.0V-1.5V (preferably-0.6V-1.1V), the scanning speed is 0.1V/s-0.5V/s (preferably 0.2V/s-0.3V/s), and the polymerization circle number is 5-15 circles (preferably 10 circles).
The mass ratio of the red monomer to the green monomer in the precursor solution is 2:3.
In the invention, a copolymer film is electrodeposited on the surface of FTO glass which is spin-coated with a polymer film in a precursor solution by adopting an in-situ electrochemical polymerization method. Electrochromic properties were further tested including spectroelectrochemical, optical contrast, transmittance.
The optical contrast of the laminated electrochromic polymer film at 520nm is 37.8%.
The application of the laminated electrochromic polymer film is that the film is used as a black display electrochromic material.
The laminated electrochromic polymer film is suitable for intelligent windows, automobile rearview mirrors, plane displays and flexible wearable equipment.
Compared with the prior art, the invention has the beneficial effects that: a method for preparing a black-high transmission reversible electrochromic material is provided, which is simple and controllable, and the prepared black-display polymer electrochromic material exhibits excellent electrochromic properties, and is expected to be used in intelligent windows, automobile rearview mirrors, flat panel displays and flexible wearable devices.
Drawings
FIG. 1 is the molecular structure of one polymer and two polymerized monomers used in examples 1 and 2;
FIG. 2 is a cyclic voltammogram of the laminated polymer film produced in example 1 at a scanning speed of 0.2V/s at-0.6 to 1.1V;
FIG. 3 is the transmittance of the laminated polymer film prepared in example 1 at various voltages;
FIG. 4 is a graph showing the transmittance over time of the laminated polymer film prepared in example 1 at a specific wavelength in a multi-potential step of from-0.2 to 0.9V;
FIG. 5 is a cyclic voltammogram of the laminated polymer film produced in example 2 at a scanning speed of 0.2V/s at-0.6 to 1.1V;
FIG. 6 is the transmittance of the laminated polymer film prepared in example 2 at various voltages;
FIG. 7 is a graph showing the transmittance over time of the laminated polymer film prepared in example 2 at a specific wavelength in a multi-potential step of from-0.2 to 0.9V.
FIG. 8 is a cyclic voltammogram of the laminated polymer film produced in example 3 at a scanning speed of 0.2V/s at-0.6 to 1.1V;
FIG. 9 is the transmittance of the laminated polymer film prepared in example 3 at various voltages;
FIG. 10 is a graph showing the transmittance over time of the laminated polymer film prepared in example 3 at a specific wavelength in a multi-potential step of from-0.2 to 0.9V.
FIG. 11 is a cyclic voltammogram of the laminated polymer film produced in example 4 at a scanning speed of 0.2V/s at-0.6 to 1.1V;
FIG. 12 is the transmittance of the laminated polymer film prepared in example 4 at various voltages;
FIG. 13 is a graph showing the transmittance over time of the laminated polymer film prepared in example 4 at a specific wavelength in a multi-potential step of from-0.2 to 0.9V.
Detailed Description
The technical scheme of the present invention is further described in the following specific examples, but the scope of the present invention is not limited thereto.
Example 1
The precursor molecular structure used is shown in figure 1. The concentration of the prepared polymer solution (I) is 6mg/mL, the concentration of the monomer solution (II) and the concentration of the monomer solution (III) are 1mg/mL, the supporting electrolyte is 0.1M tetrabutylammonium hexafluorophosphate, and the electrolytic solvent is a mixed solvent of dichloromethane and acetonitrile with the volume ratio of 3:2. Preparation of a laminated polymer film: uniformly dripping the polymer solution (I) on FTO conductive glass, and preparing a polymer film by spin coating through a spin coater; secondly, taking a solution with the mass ratio of 3:2 from a monomer solution (II) and a monomer solution (III) to prepare a precursor solution of a red monomer and a green monomer; then, a laminated polymer film is prepared in a precursor solution by a cyclic voltammetry polymerization method under the following polymerization conditions: -0.6V-1.1V, scanning rate of 0.2V/s, number of polymerization turns of 10. Electrochromic Property test of copolymer film: the stability of the films was tested using cyclic voltammetry in a 0.1M solution of tetrabutylammonium hexafluorophosphate in acetonitrile and the data processing results are shown in FIG. 2. The prepared films were tested for uv-vis absorption at different voltages and transmittance at specific wavelengths as a function of time in a 0.1M tetrabutylammonium hexafluorophosphate/acetonitrile solution using an electrochemical workstation and uv-vis spectrophotometer, and the data processing results are shown in fig. 3 and 4.
Example 2
The precursor molecular structure used is shown in figure 1. The concentration of the prepared polymer solution (I) is 10mg/mL, the concentration of the monomer solution (II) and the concentration of the monomer solution (III) are 5mg/mL, the supporting electrolyte is 0.1M tetrabutylammonium hexafluorophosphate, and the electrolytic solvent is a mixed solvent of dichloromethane and acetonitrile with the volume ratio of 3:2. Preparation of a laminated polymer film: uniformly dripping the polymer solution (I) on FTO conductive glass, and preparing a polymer film by spin coating through a spin coater; secondly, taking a solution with the mass ratio of 3:2 from a monomer solution (II) and a monomer solution (III) to prepare a precursor solution of a red monomer and a green monomer; then, a laminated polymer film is prepared in a precursor solution by a cyclic voltammetry polymerization method under the following polymerization conditions: -0.6V-1.1V, scanning rate of 0.2V/s, number of polymerization turns of 10. Electrochromic Property test of copolymer film: the stability of the films was tested using cyclic voltammetry in a 0.1M solution of tetrabutylammonium hexafluorophosphate in acetonitrile and the data processing results are shown in FIG. 5. The prepared films were tested for uv-vis absorption at different voltages and transmittance at specific wavelengths versus time, respectively, in 0.1M tetrabutylammonium hexafluorophosphate/acetonitrile solution using an electrochemical workstation and uv-vis spectrophotometer, and the data processing results are shown in fig. 6 and 7.
Example 3
The precursor molecular structure used is shown in figure 1. The concentration of the prepared polymer solution (I) is 1mg/mL, the concentration of the monomer solution (II) and the concentration of the monomer solution (III) are 0.5mg/mL, the supporting electrolyte is 0.1M tetrabutylammonium hexafluorophosphate, and the electrolytic solvent is a mixed solvent of dichloromethane and acetonitrile with the volume ratio of 3:2. Preparation of a laminated polymer film: uniformly dripping the polymer solution (I) on FTO conductive glass, and preparing a polymer film by spin coating through a spin coater; secondly, taking a monomer solution (II) and a monomer solution (III) to prepare a precursor solution of a red monomer and a green monomer, wherein the mass ratio of the monomer solution to the monomer solution (III) is 2:3; then, a laminated polymer film is prepared in a precursor solution by a cyclic voltammetry polymerization method under the following polymerization conditions: -0.6V-1.1V, scanning rate of 0.2V/s, number of polymerization turns of 10. Electrochromic Property test of copolymer film: the stability of the films was tested using cyclic voltammetry in a 0.1M solution of tetrabutylammonium hexafluorophosphate in acetonitrile and the data processing results are shown in FIG. 8. The prepared films were tested for uv-vis absorption at different voltages and transmittance at specific wavelengths as a function of time in a 0.1M tetrabutylammonium hexafluorophosphate/acetonitrile solution using an electrochemical workstation and uv-vis spectrophotometer, and the data processing results are shown in fig. 9 and 10.
Example 4
The precursor molecular structure used is shown in figure 1. The concentration of the prepared polymer solution (I) is 6mg/mL, the concentration of the monomer solution (II) and the concentration of the monomer solution (III) are 1mg/mL, the supporting electrolyte is 0.1M tetrabutylammonium hexafluorophosphate, and the electrolytic solvent is a mixed solvent of dichloromethane and acetonitrile with the volume ratio of 3:2. Preparation of a laminated polymer film: uniformly dripping the polymer solution (I) on FTO conductive glass, and preparing a polymer film by spin coating through a spin coater; secondly, taking a solution with the mass ratio of 1:1 from the monomer solution (II) and the monomer solution (III) to prepare a precursor solution of a red monomer and a green monomer; then, a laminated polymer film is prepared in a precursor solution by a cyclic voltammetry polymerization method under the following polymerization conditions: -0.6V-1.1V, scanning rate of 0.2V/s, number of polymerization turns of 10. Electrochromic Property test of copolymer film: the stability of the films was tested using cyclic voltammetry in a 0.1M tetrabutylammonium hexafluorophosphate/acetonitrile solution and the data processing results are shown in FIG. 11. The prepared films were tested for uv-vis absorption at different voltages and transmittance at specific wavelengths as a function of time in a 0.1M tetrabutylammonium hexafluorophosphate/acetonitrile solution using an electrochemical workstation and uv-vis spectrophotometer, and the data processing results are shown in fig. 12 and 13.
Claims (10)
1. A black-high transmission reversibly switchable laminated polymer film prepared by the method of: firstly, preparing a polymer solution (I) with the concentration of 1-10 mg/mL, uniformly dripping the polymer solution (I) onto FTO conductive glass, and preparing a polymer film by spin coating through a spin coater; secondly, preparing a monomer solution (II) and a monomer solution (III) with the concentration of 0.5-5 mg/mL; then, taking a solution with the mass ratio of 2:3-3:2 from the monomer solution (II) and the monomer solution (III) to prepare a precursor solution of a red monomer and a green monomer; finally, electrodepositing a layer of copolymer film on the FTO conductive glass spin-coated with the polymer film in the precursor solution by using a cyclic voltammetry polymerization method;
。
2. a black-highly transmissive reversible switching laminated polymer film according to claim 1, wherein the polymer exhibiting violet color is formulated with an electrolytic solvent to give a polymer solution designated as polymer solution (i); uniformly dripping the polymer solution (I) on FTO conductive glass, and preparing a polymer film by spin coating through a spin coater; in a three-electrode system using FTO conductive glass spin-coated with a polymer film as a working electrode, a platinum wire as a counter electrode and an Ag/AgCl electrode as a reference electrode, two polymerization precursors respectively showing red and green, a supporting electrolyte and an electrolytic solvent are used to prepare two monomer solutions, which are respectively named monomer solution (II) and monomer solution (III).
3. A black-high transmission reversible switching laminated polymer film according to claim 2, wherein said polymer solution is formulated to have a polymer concentration of 1 to 10mg/mL; in the prepared monomer solution, the concentration of the monomer is 0.5-5 mg/mL, and the concentration of the supporting electrolyte is 0.05-0.3 mol/L.
4. A method for preparing a black-high transmission reversible transition laminated polymer film according to claim 1, wherein the preparation method is carried out as follows: firstly, preparing a polymer solution (I) with the concentration of 1-10 mg/mL, uniformly dripping the polymer solution (I) onto FTO conductive glass, and preparing a polymer film by spin coating through a spin coater; secondly, preparing a monomer solution (II) and a monomer solution (III) with the concentration of 0.5-5 mg/mL; then, taking a solution with the mass ratio of 2:3-3:2 from the monomer solution (II) and the monomer solution (III) to prepare a precursor solution of a red monomer and a green monomer; finally, electrodepositing a layer of copolymer film on the FTO conductive glass spin-coated with the polymer film in the precursor solution by using a cyclic voltammetry polymerization method;
。
5. the method for producing a black-high transmittance reversible switching laminated polymer film according to claim 4, wherein the spin-coating time of the spin coater is 60s.
6. The method for producing a black-high transmittance reversible switching laminated polymer film according to claim 4, wherein the mass ratio of the red monomer to the green monomer in the precursor solution is 2:3.
7. The method for producing a black-high transmission reversible transition laminated polymer film according to claim 4, wherein the number of cyclic voltammetry polymerization turns is 10.
8. The method of preparing a black-high transmission reversibly switchable laminated polymeric film according to claim 4, wherein the film is rendered black in a neutral state and transparent in an oxidized state; the film exhibits high optical contrast.
9. Use of a black-high transmission reversibly switchable laminated polymer film according to claim 1, wherein the film is used as an electrochromic material for black displays.
10. The use according to claim 9, wherein the laminated polymer film electrochromic material is suitable for use in smart windows, automotive rearview mirrors, flat panel displays and flexible wearable devices.
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